Crosslinked carboxymethyl starch (cCMS) hydrogels were synthesized in a simple one step process using various crosslinking agent content – dichloroacetic acid (DCA) with the constant monochloroacetic acid and DCA/anhydroglucosidic unit (AGU) 1.75:1 molar ratio whereas DCA/AGU was changed in a range 0.15–1.0 mol/AGU. The degree of substitution (DS = 0.4–0.9), and reaction efficiency were evaluated. Moreover, swellability in water and aqueous solutions was determined. Adsorption tests for Fe(II) cation as a function of cCMS crosslinking degree, sorbent dose and time were performed in autogenic pH (ca. 7.0). For comparison four other divalent metal cations were tested. Adsorption efficiency was up to 98% for Fe(II), 96% for Ca(II) and above 99.7% for Cu(II), Cd(II) and Pb(II).